Method of obtaining titanic oxid.



-- 1,106,409.. R o Drawing.

AUeUsrE J, ROSSI AND Louis E.

' UNITED STATES A. CORPORATION OF MAINE.

PATENT OFFICE.

BARTON, or NIAGARA FALLS, NEW YORK, ASSIGN- ons'ro THE TITANIUM ALLOY MANUFACTURING COMPANY, or NEW YORK, N. Y.,

METHOD OF OBTAINING TITANIC OXID.

To all whom it may 0.3mm.-

Be it known that We, AUGUSTE J. Rossi and Lows E. BARTON, both citizens of the YUnite'd States, and residents of Niagara Falls, in the county of Niagara and State of New York, have .jointly invented certain new and useful Improvements in Methods of Obtaining Titanic Oxid," of which the fol comparatively high percentages of iron oxid,

as for example ordinary titaniferous iron, or ilmenite, ores, as distinguished from such substances containing low percentages of iron oxid and known for example as Frutile ores.

w The object of our invention comprise provision of a novel, industrially practicable, method, whereby, from such substances, may

be obtained, at less cost, loss, labor and skill,

and'with greater certainty than formerly, concentrate products containing exception- I ally high percentage of titanic oxid, and exceptionally low, if any, percentages of iron oxid or other undesirable substances, and

possessing alsoproperties especially adapting them for certain uses.

We havediscovered that, by, as a preliminary step, charging and melting, together with said substances, sulfid of an alkall 'metalas such, preferably sodium sulfid or potassium sulfid, the resulting fusion and melt is distinguished by novel reactions and characteristics by. aid of which attainment of our said objects is facilitated and otherwise promoted.

Our novel method is, for'gexample, practised as follows: Into a'furnace, provided with refractory. linings and capable. of developing and maintaining requisite tempera] ture, we charge" titaiiiferous iron oie yand,

preferably, sodium sulfid, preferably; intimately mixed, and h afi-ithe'same until thoroughly melted. The proportion ofthe sul fid of 'the alkali metal-should be somewhat excess of enough to insure formation offerrous sulfid from all the iron constituents of the'ore; oftitanateof the alkali metal from' all'the' titanifim constituents, and of alkali silicates and aluminates from silica-and alfimifiaof the g s e, such P P particular ore treated. We. have, for v ex ample, 1n treatlng an ore containing about portioned as follows, viz

.Ore! 100 parts. Sodium sulfid 100 parts.

This charge gave us good results, the sodium sulfid being present as aforesaid in excess. We believe that during this melt-the following reactions principally occurred any convenient manner as by tapping. or pouring. The melt is of exceptionally desirable consistency and quality. Though it comes from the furnace as a molten slag capable of being cast and solidified into a solid mass, it is comminutable with exceptional ease, and, if crushed to only about one-quarterinch mesh, will, after one or two days exposure to-the atmosphere, disintegrate into a fine powder very serviceable for our purmediat'ely after cooling, its nature and consistency is suchas to admit of its immediate successfuluse in that form in the hereafterdescribed next following step of our process. We lixiviate our said melt with water. We believe that, during the lixiviation, the following reactions occur. (1) Excess sodium salts dissolve; (2) much iron passes into solution as a ferro sodium sulfid; .(3) sodium titanate is decomposed, formin'g hydrated titanic oxid and sodium hydrate;

(4:) sodium silicate and sodium aluminate are dissolved.

nature and consistency of our'melt,-iope'r.- ates to dissolve' mos't of the salts, and then in'g' completion of the decomposition of the ti'tana'te. For economy, this resulting solution may, as 'will be understood; be readily freedfrom'its'impuritiesand the salts rethe i nelt, z. e.- the' undis solved constitutents ing readily calculated from analysis of the;

42% iron oxid and 52% titaniumoxid'prm' The melt is removed from the furnace in poses. On the other hand, if so crushed im-- Yrwe finally lixiviate .with hot or, boiling ,watergthis ;bein'g"for the purpose of hasten covered in form suitable for use in smelting the next ,chargeof ore.- The rema nder of;

Specification of Letters Patent. Patented Aug. 11, 1914. I Application filed February s, 1913. Serial No. 746,567.-

. v We preferto lixiviate first withcold, or merely warm, water, which, owing tothe' account of its comparative cheapness, but

other acids capable, at the same degree of.

dilution, of dissolving iron sulfid, such for example as hydrochloric acid, may be,

though less economically, employed; The

proportion of sulfuric, or other, acid thus employed should be calculated from analysis of the residues of the melt insoluble in water. For example, in approximately the ratio of 1.75 parts of sulfuric acid to 1 part oussubstance and the sulfid ofthe alkali.

' prepare our said metal, lixiviatin of metallic iron, the said acid beingdiluted by four times its weight of water in thebath. We prefer however to proportion the acid relatively to the iron somewhat in excess, in order to neutralize any small quantities of sodium compounds, including titanate, which may have escaped the lixiviation with water. Our last aforesaid insoluble residue we then calcine after washing it with water, the resultingfinal product being substantially pure titanic oxid in the form of an amorphous, smooth, soft, white powder, characterized as containing, therewith commingled, traces, or not to exceed one .per cent. of iron oxid.

It will be understood that while we prefer to preliminarily mix together the titanifermetal beforechargmg and melting, the said mix'ng might, though unpreferably, be accomplished in any order, or at, any'stagp, of the single operation or heat by"'wh ic we melt; without departing from our invention.

What we claim as new and desire to secure by \Letters Patent is the following, viz

1. The method of obtaining titanic oxid from a substance containing it and iron oxid which comprises charging and meltin to gether with said substance sulfid of an a ali the resulting melt with water, withdrawm the undissolved portion of said melt, and oiling it in a bath containing acid so'dilute as to dissolve the there-- in iron; but not the therein pounds.

2. The method of obtaining titanic, oxid titanium, comfrom a substance containing it and iron oxid which comprises 'cliarging and. melting 120-.

gether with said substance sodium sulfid,

lixiviating the resulting melt with water-,-

withdrawing the undissolved portion of said melt, and boiling it in a bath containing acid so dilute as to dissolve the therein iron, but not the therein titanium, compounds.

3. The method of obtaining titanic oxid from a substance containing it and iron oxid 4. The method of obtaining. titanic Oedfrom'a substance containing it and iron oxid which comprises charging and melting together with said substance .sodium sulfid, lixiviating the resulting melt, with water, withdrawing the undissolved portion of said melt, and boilingit in a bath containing sulfur'ic acid so dilute as to dissolve the therein iron, but not the therein titanium, compounds; a r

5. The method of obtaining titanic oxid from a substance containing it and iron oxid whichcomprises charging and melting together with said substance sulfid of an alkali metal, lixiviating the resulting meltwith water, withdrawlng the undissolved portion of said melt, boiling it in a bath containing acid so dilute as to dissolve the therein iron, but not the therein titanium, compounds, and calcining the undissolved residue. 4 i 4 6. The method of obtaining titanic'oxid from a substance containing it and iron oxid which comprises chargingand melting together with said substance sodium sulfid,- lixiviating the resulting melt with withdrawing the undissolvedv portion melt, boiling it in a bath containin acid-so dilute as to dissolve the therein 1ron, but not the therein titanium, compounds, and calcining the undissolved residue.

7. The method of obtaining titanic oxid from a substance containing it and iron oxid which'comprises charging and melting to-' of said gether with said substance sulfid of an alkali metal, lixiviating the resulting melt with water, withdrawing the undissolved portion of said melt. boiling it in a bath containing sulfuric acid so dilute as compounds, and calcining the 'undissolved residue. I

8. The'method of obtainingtitanic oxid from; a substance containing it and iron oxid withdrawlng the undissolved portion of said to dissolve vthe therein iron, but not the therein titanium,.

water,

said substance sodium sulfid,

melt, boiling. it ina bath containing sul-I' t erein furic acid so dilute as to dissolve the iron, but not the therein titanium,. com-1" pounds, and calcining the undissolved resldue.

9. In obtaining titanic oxid from a substance containing it and iron oxid the 'steps which consist in making, in one operation or heat, a melt from sulfid of an alkali; metal charged ,as such together with said substance and thereafter lixiviating the resulting melt and thereafter lixiviating the resulting melt With Water.

,. with water.

10. In obtaining titanic oxid from a substance containing it and iron oxid the steps 1 which consist in nmaking, in one operation Witnesses: v v

01' heat, a melt from sulfid of sodium WALTER D. EnMoNns, charged as such together with said substance PHILIP C. PEoK. 

